CN104364861B - Anti-flammability electrolytic capacitor - Google Patents
Anti-flammability electrolytic capacitor Download PDFInfo
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- CN104364861B CN104364861B CN201380030513.0A CN201380030513A CN104364861B CN 104364861 B CN104364861 B CN 104364861B CN 201380030513 A CN201380030513 A CN 201380030513A CN 104364861 B CN104364861 B CN 104364861B
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- electrolytic capacitor
- branched
- straight
- electrolyte
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- 239000003990 capacitor Substances 0.000 title claims abstract description 85
- -1 ester amides Chemical class 0.000 claims abstract description 83
- 239000003792 electrolyte Substances 0.000 claims abstract description 66
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011888 foil Substances 0.000 claims abstract description 25
- 125000003709 fluoroalkyl group Chemical group 0.000 claims abstract description 18
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 15
- 230000004888 barrier function Effects 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 229910019142 PO4 Inorganic materials 0.000 claims description 26
- 239000010452 phosphate Substances 0.000 claims description 26
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 abstract description 59
- 230000000694 effects Effects 0.000 abstract description 19
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 13
- 239000008151 electrolyte solution Substances 0.000 abstract description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 101
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- 150000003863 ammonium salts Chemical class 0.000 description 3
- 238000003491 array Methods 0.000 description 3
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- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
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- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 3
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- 238000012545 processing Methods 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
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- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical class CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 description 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
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- 229920000305 Nylon 6,10 Polymers 0.000 description 1
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- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
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- 230000000996 additive effect Effects 0.000 description 1
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- 235000011037 adipic acid Nutrition 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003282 alkyl amino group Chemical group 0.000 description 1
- 125000004414 alkyl thio group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000019437 butane-1,3-diol Nutrition 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000003950 cyclic amides Chemical class 0.000 description 1
- KTHXBEHDVMTNOH-UHFFFAOYSA-N cyclobutanol Chemical compound OC1CCC1 KTHXBEHDVMTNOH-UHFFFAOYSA-N 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- XCIXKGXIYUWCLL-UHFFFAOYSA-N cyclopentanol Chemical compound OC1CCCC1 XCIXKGXIYUWCLL-UHFFFAOYSA-N 0.000 description 1
- YSRSBDQINUMTIF-UHFFFAOYSA-N decane-1,2-diol Chemical compound CCCCCCCCC(O)CO YSRSBDQINUMTIF-UHFFFAOYSA-N 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229940113088 dimethylacetamide Drugs 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical class CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 description 1
- AJFDBNQQDYLMJN-UHFFFAOYSA-N n,n-diethylacetamide Chemical class CCN(CC)C(C)=O AJFDBNQQDYLMJN-UHFFFAOYSA-N 0.000 description 1
- DAZXVJBJRMWXJP-UHFFFAOYSA-N n,n-dimethylethylamine Chemical compound CCN(C)C DAZXVJBJRMWXJP-UHFFFAOYSA-N 0.000 description 1
- ZWRUINPWMLAQRD-UHFFFAOYSA-N n-Nonyl alcohol Natural products CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 1
- MWKFXSUHUHTGQN-UHFFFAOYSA-N n-decyl alcohol Natural products CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 1
- KERBAAIBDHEFDD-UHFFFAOYSA-N n-ethylformamide Chemical class CCNC=O KERBAAIBDHEFDD-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- XUZLXCQFXTZASF-UHFFFAOYSA-N nitro(phenyl)methanol Chemical compound [O-][N+](=O)C(O)C1=CC=CC=C1 XUZLXCQFXTZASF-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluic acid Chemical compound CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000003053 piperidines Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000029219 regulation of pH Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229960005137 succinic acid Drugs 0.000 description 1
- VACCAVUAMIDAGB-UHFFFAOYSA-N sulfamethizole Chemical compound S1C(C)=NN=C1NS(=O)(=O)C1=CC=C(N)C=C1 VACCAVUAMIDAGB-UHFFFAOYSA-N 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical class CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical class OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention is provided can also keep the anti-flammability electrolytic capacitor of flame retardant effect after long-time.The anti-flammability electrolytic capacitor has：The anode foils of oxide film thereon, Cathode Foil, barrier film and the electrolyte containing solute in a solvent are provided with the surface, wherein, in the electrolytic solution containing the phosphoric ester amides represented by following formulas (1), in formula, n is 1 or 2, R1And R2Alkyl of the carbon number for 1~10 straight or branched is separately represented, Rf represents the alkyl of the straight or branched for being 1~10 containing fluoroalkyl or carbon number for the straight or branched that carbon number is 1~10.
Description
Technical field
The present invention relates to electrolytic capacitor, the electricity of good anti-flammability can be also kept more particularly to after long-time
Electrolysis condenser.
Background technology
Electrolytic capacitor has small-sized, Large Copacity feature, is used as the composition of various electronic equipments, vehicle boarded equipment etc.
One of part is widely used.Electrolytic capacitor possesses：On the surface with the anode foils of oxide film thereon, Cathode Foil and every
Film, with will be clipped between anode foils and Cathode Foil they are wound in the state of barrier film obtained from element be impregnated in electrolysis
Structure in liquid.Here, as electrolyte, being dissolved using in the flammable organic solvent such as ethylene glycol, gamma-butyrolacton
Solution obtained from boric acid, carboxylic acid or its ammonium salt etc..
Therefore, apply excessive electric stress to electrolytic capacitor and during safety valve startup, it is possible to because being produced by short circuit etc.
Raw spark and the electrolyte after gasification is caught fire so that member combusts.Thus, studying to assign electrolytic capacitor always and hindering
Combustion property.
Patent document 1, Patent Document 2 discloses using anti-flammability barrier film method.Although this method can suppress electricity
The burning of electrolysis condenser itself, but be difficult to the bath composition sprayed from safety valve is fire-retardant.On the other hand, patent document 3, specially
The addition phosphate such as trimethyl phosphate or triethyl phosphate in the electrolytic solution is disclosed in sharp document 4 and anti-flammability, suppression is assigned
The technology of the burning of bath composition.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 5-243089 publications
Patent document 2：Japanese Unexamined Patent Publication 2011-129773 publications
Patent document 3：Japanese Unexamined Patent Publication 1-95512 publications
Patent document 4：Japanese Unexamined Patent Publication 3-180014 publications
The content of the invention
Invent problem to be solved
Generally, electrolytic capacitor is manufactured under atmospheric pressure, but the natural fiber and electrolyte used as barrier film has suction
Receive the property of the moisture in air.Therefore, in the case of the solution without addition water is used as electrolyte, after manufacture
The element of electrolytic capacitor usually contain moisture.In the past, the trimethyl phosphate or triethyl phosphate that are used as fire retardant with
Reaction of moisture in element, easily causes hydrolysis.Therefore, trimethyl phosphate or triethyl phosphate occur to divide after long-time
, there is the problem of can not playing flame retardant effect in solution.
The present invention be in view of above-mentioned problem and complete, its object is to there is provided with good anti-flammability, through it is long when
Between after can also keep the anti-flammability electrolytic capacitor of flame retardant effect.
Means for solving the problems
The present inventors have been repeated in-depth study, as a result found, by electrolyte to solve above-mentioned problem
In contain phosphoric ester amides, electrolytic capacitor has good anti-flammability, by long-time can also keep good fire-retardant effect
Really, in addition, significantly improving voltage-resistent characteristic, so as to complete the present invention.
That is, anti-flammability electrolytic capacitor of the invention has：Anode foils, the negative electrode of oxide film thereon are provided with the surface
Paper tinsel, barrier film and the electrolyte containing solute in a solvent, it is characterised in that contain in above-mentioned electrolyte by following formulas (1)
Or the phosphoric ester amides that following formulas (2) represent.
(in formula, n is 1 or 2, R1And R2Separately represent alkyl of the carbon number for 1~10 straight or branched.
Rf represents the alkane of the straight or branched for being 1~10 containing fluoroalkyl or carbon number for the straight or branched that carbon number is 1~10
Base.)
(in formula, n is 1 or 2, A represent polymethylene that polymethylene, carbon number that carbon number is 4~7 are 4~7
In at least one positions of C-C keys form the groups of C-O-C keys, carbon number for the C-C keys in 4~7 polymethylene extremely
Few 1 position forms at least one position of the group or carbon number of C-NH-C keys for the C-C keys in 4~7 polymethylene
Form C-N (CH3)-C keys group.Rf represents that carbon number contains fluoroalkyl or carbon number for 1~10 straight or branched
For the alkyl of 1~10 straight or branched.)
In addition, the anti-flammability electrolytic capacitor of the present invention is characterised by, in the electrolytic solution containing by following formulas (3) or
The phosphoric ester amides that following formulas (4) represent.
(in formula, R1’And R2’Separately represent alkyl of the carbon number for 1~10 straight or branched.Rf’Represent
Carbon number contains fluoroalkyl for 1~10 straight or branched.)
(in formula, A represents the C-C keys in the polymethylene that the polymethylene that carbon number is 4~7, carbon number are 4~7
At least one position form at least one position of the groups of C-O-C keys, carbon number for the C-C keys in 4~7 polymethylene
Form the group or carbon number of C-NH-C keys and form C-N at least one position of the C-C keys in 4~7 polymethylene
(CH3)-C keys group.Rf’Represent that carbon number contains fluoroalkyl for 1~10 straight or branched.)
Additionally, it is preferred that integrally any into (4) by above-mentioned formula (1) containing 5~30 weight % relative to electrolyte
The phosphoric ester amides of one expression.
In addition, the anti-flammability electrolytic capacitor of the present invention can also contain by following formulas (5) table in above-mentioned electrolyte
The di-phosphate ester anion shown.
(in formula, Rf1And Rf2Represent the straight or branched that carbon number is 1~10 is 1 containing fluoroalkyl or carbon number
The alkyl of~10 straight or branched.)
Additionally, it is preferred that relative to electrolyte integrally containing 0~50 weight % by above-mentioned formula (5) represent di-phosphate ester
Anion.
And then, the moisture content in anti-flammability electrolytic capacitor preferred element of the invention is below 10 weight %.
Invention effect
In accordance with the invention it is possible to which providing is improved with good anti-flammability, voltage-resistent characteristic and by for a long time
The electrolytic capacitor of good flame retardant effect is also kept afterwards.
And then, electrolytic capacitor of the invention can also play fire-retardant in the case of using the electrolyte containing water
Effect, therefore, it is possible to provide the electrolytic capacitor that equivalent series resistance (ESR) is low.
Embodiment
The electrolytic capacitor of the present invention is in the electrolytic solution containing the phosphoric ester amides represented by above-mentioned formula (1) to (4).Can
There are 1 or 2 acid amides positions with the phosphoric ester amides for thinking formula (1) to (4), pass through its electro and three-dimensional effect
Really, phosphoric ester amides have and are difficult to by the property hydrolyzed.Therefore, by making it contain in the electrolytic solution, it can obtain long-term
Keep the electrolytic capacitor of anti-flammability.
In addition, by being bonded fluorine atom in the ester side chain of phosphoric ester amides, showing just to show with a small amount of addition
The excellent flame retardant effect such as flame retardant effect, can obtain the anti-flammability electrolytic capacitor with good characteristic.
And then, although the mechanism of action is indefinite, but by containing the phosphoric ester amides of formula (1) to (4) in the electrolytic solution,
The effect that the proof voltage of electrolytic capacitor is significantly improved can be assigned.
(phosphoric ester amides)
In formula (1), n is 1 or 2, R1And R2It is 1~10 straight or branched separately to represent carbon number
Alkyl.Wherein, R1And R2Can by alkoxy, hydroxyl, amino, N- alkyl aminos, N, N- dialkyl amidos, fluorine atom aryl,
The substituent such as alkylthio group and itrile group replaces.Rf represents the former containing fluoroalkyl or carbon of the straight or branched that carbon number is 1~10
Subnumber is the alkyl of 1~10 straight or branched.
It is used as R1And R2, for example, can include：Methyl, ethyl, n-propyl, isopropyl, normal-butyl, sec-butyl, uncle
Butyl, n-pentyl, n-hexyl, n-octyl, positive decyl etc..It is used as the R after being substituted with a substituent1And R2, for example, can enumerate
Go out：2- methoxy ethyls, 2- hydroxyethyls, 2- amino-ethyls, 2- (N- methylaminos) ethyl, 2- (N, N- dimethylamino) second
Base, 2- phenylethyls, 2- methyl thioethyls, 2- cyano ethyls etc..As Rf, for example, can include：Methyl, ethyl, positive third
Base, isopropyl, normal-butyl, sec-butyl, the tert-butyl group, n-pentyl, n-hexyl, n-octyl, positive decyl, trifluoromethyl, 2- fluoro ethyls,
The fluoro ethyls of 2,2- bis-, 2,2,2- trifluoroethyls, the fluoropropyls of 2,2,3,3- tetra-, the fluoropropyls of 2,2,3,3,3- five, hexafluoro isopropyl, 2,
2,3,3,4,4,5,5- octafluoros amyl group, the difluoro heptyl of 2,2,3,3,4,4,5,5,6,6,7,7- ten, 3,3,4,4,5,5,6,6,7,
Fluorine decyls of 7,8,8,9,9,10,10,10- 17 etc..
As the phosphoric ester amides of formula (1), as n=1 example, it can include：Dimethyl phosphate diethyl acyl
Double (trifluoromethyl ester) diethylamides of amine, phosphoric acid, diethyl phosphate diethylamide, double (2,2,2- trifluoro ethyl esters) diformazans of phosphoric acid
Double (2,2,2- trifluoro ethyl esters) diethylamides of base acid amides, phosphoric acid, phosphoric acid double (2,2,2- trifluoro ethyl esters) diη-propyl acid amides, phosphorus
Double (2,2,2- trifluoro ethyl esters) the di-n-butyl acid amides of sour double (2,2,2- trifluoro ethyl esters) diisopropylamides, phosphoric acid, phosphoric acid it is double (2,
2,2- trifluoro ethyl esters) di-sec-butyl acid amides, double (2,2,2- trifluoro ethyl esters) di-te t-butylamides of phosphoric acid, the double (2,2,2- tri- of phosphoric acid
Fluorine ethyl ester) di-n-hexyl acid amides, double (2,2,2- trifluoro ethyl esters) the di-n-octyl acid amides of phosphoric acid, phosphoric acid is double (2,2,2- trifluoro ethyl esters)
Double (2,2,2- trifluoro ethyl esters) ethylmethyl amides of two positive decyl acid amides, phosphoric acid, double (the 2,2,3,3- tetrafluoros propyl ester) diethyls of phosphoric acid
Double (the fluorine propyl ester of the 2,2,3,3,3- five) diethylamides of base acid amides, phosphoric acid, phosphoric acid are double (2,2,3,3,4,4,5,5- octafluoros pentyl ester)
Double (the fluorine pentyl esters of the 2,2,3,3,4,4,5,5,5- nine) diethylamides of diethylamide, phosphoric acid, phosphoric acid it is double (2,2,3,3,4,4,5,
The difluoro heptyl esters of 5,6,6,7,7- ten) diethylamide, the double (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10- of phosphoric acid
17 fluorine last of the ten Heavenly stems esters) diethylamide etc..As n=2 example, it can include：Phosphoric acid double (diethylamide) methyl esters, phosphoric acid
Double (diethylamide) ethyl esters of double (diethylamide) trifluoromethyl esters, phosphoric acid, double (dimethylformamide) 2,2,2- trifluoro second of phosphoric acid
Double (diethylamide) the 2,2,2- trifluoro ethyl esters of ester, phosphoric acid, double (diη-propyl acid amides) the 2,2,2- trifluoro ethyl esters of phosphoric acid, phosphoric acid are double
Double (di-n-butyl acid amides) the 2,2,2- trifluoro ethyl esters of (diisopropylamide) 2,2,2- trifluoro ethyl esters, phosphoric acid, double (the di-secondary fourths of phosphoric acid
Base acid amides) 2,2,2- trifluoro ethyl esters, double (di-n-hexyl acid amides) the 2,2,2- trifluoro ethyl esters of phosphoric acid, phosphoric acid is double (di-n-octyl acid amides)
Double (two positive decyl acid amides) the 2,2,2- trifluoro ethyl esters of 2,2,2- trifluoro ethyl esters, phosphoric acid, double (ethylmethyl amide) 2,2,2- of phosphoric acid
Double (diethylamide) the 2,2,3,3- tetrafluoros propyl ester of trifluoro ethyl ester, phosphoric acid, double (diisopropylamide) the 2,2,3,3- tetrafluoros of phosphoric acid
The double fluorine propyl ester of (diethylamide) 2,2,3,3,3- five of propyl ester, phosphoric acid, double (diethylamide) 2,2,3,3,4,4,5,5- of phosphoric acid
The double difluoro heptyl esters of (diisopropylamide) 2,2,3,3,4,4,5,5,6,6,7,7- ten of octafluoro pentyl ester, phosphoric acid, the double (diethyl of phosphoric acid
Acid amides) 17 fluorine last of the ten Heavenly stems esters etc. of 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-.
In formula (2), n be 1 or 2, A represent polymethylene, carbon number that carbon number is 4~7 be 4~7 it is more sub-
It is the C-C keys in 4~7 polymethylene that at least one position of C-C keys in methyl, which forms the group of C-O-C keys, carbon number,
At least one position formed C-NH-C keys group or carbon number for 4~7 polymethylene in C-C keys at least one
Position forms C-N (CH3)-C keys group.Rf represents that carbon number contains fluoroalkyl for 1~10 straight or branched.
As the phosphoric ester amides of formula (2), as n=1 example, it can include：Double (the 2,2,2- of phosphinylidyne pyrrolidines
Trifluoro ethyl ester), phosphinylidyne piperidines double (2,2,2- trifluoro ethyl esters), phosphinylidyne hexamethylene imine double (2,2,2- trifluoro ethyl esters), phosphinylidynes
Heptamethylene imines double (2,2,2- trifluoro ethyl esters), phosphinylidyne morpholine double (2,2,2- trifluoro ethyl esters), the double (2,2,2- tri- of phosphinylidyne piperazine
Fluorine ethyl ester), phosphinylidyne N '-methyl piperazine double (2,2,2- trifluoro ethyl esters) etc..As n=2 example, it can include：Phosphinylidyne is double
Double (hexamethylene imine) the 2,2,2- trifluoros of pyrrolidines 2,2,2- trifluoro ethyl esters, phosphinylidyne bipiperidine 2,2,2- trifluoro ethyl esters, phosphinylidyne
Double (heptamethylene imines) the 2,2,2- trifluoro ethyl esters of ethyl ester, phosphinylidyne, the double morpholine 2,2,2- trifluoro ethyl esters of phosphinylidyne, phosphinylidyne BISPIP 2,
Double (N '-methyl piperazine) 2,2,2- trifluoro ethyl esters of 2,2- trifluoro ethyl esters, phosphinylidyne etc..
In the phosphoric ester amides of formula (1) or formula (2), in terms of the anti-flammability of electrolytic capacitor, the preferred n=of difference
1 and Rf is the situation containing fluoroalkyl, in aspect of performances such as the ESR of anti-flammability and electrolytic capacitor, particularly preferred phosphoric acid it is double (2,
2,2- trifluoro ethyl esters) double (2,2,2- trifluoro ethyl esters) diisopropylamides of diethylamide and phosphoric acid.
(addition)
The addition of the fluorine-containing phosphate ester acid amides of formula (1) to (4) is not particularly limited, integrally preferred relative to electrolyte
For the scope of 5~30 weight % scope, more preferably 10~20 weight %.Fire retardant is overall relative to electrolyte to be added
When dosage is more than 30 weight %, it is possible to which the resistivity rising or fire retardant for making electrolyte are difficult to dissolve in the electrolytic solution, less than 5
During weight %, it is impossible to obtain sufficient flame retardant effect.
(solvent)
As the solvent of the electrolyte of the electrolytic capacitor for the present invention, protic polar solvent, non-matter can be used
Sub- property polar solvent and their mixture.As protic polar solvent, it can include：Unary alcohol (ethanol, third
Alcohol, n-butyl alcohol, 2- butanol, amylalcohol, 3- methyl-1-butanols, hexanol, 2- methyl-1-pentenes alcohol, 3- methyl-1-pentenes alcohol, 2- methyl-
1- amylalcohols, 3- methyl-1-pentenes alcohol, 4- methyl -2- amylalcohols, 1- octanols, sec-n-octyl alcohol, 1 nonyl alcohol, 1- decyl alcohol, cyclobutanol, cyclopentanol,
Cyclohexanol, benzylalcohol etc.), polyalcohols and keto-alcohol compounds (ethylene glycol, propane diols, 1,3 butylene glycol, 1,2- penta 2
Alcohol, 2- methylpentane -2,4- glycol (hexylene glycol), 2- ethyl -1,3- hexylene glycols, TMPD, 2- methyl-2-propyls -
1,3- pentanediols, Decane-1,2-diol, glycerine, 1,2,4- butantriols, 1,2,6- hexanetriols, methyl cellosolve, ethyl cellosolve, 2-
Methoxyl group-n-butyl alcohol, 3- methoxyl groups-n-butyl alcohol, ethylene glycol list isobutyl ether, ethylene glycol mono hexyl ether, diethylene glycol, diethyl two
Alcohol list n-butyl ether, diethylene glycol monohexyl ether, triethylene glycol monoethyl ether, triethylene glycol monoisopropyl ether, triethylene glycol list
Butyl ether, MPEG, dimethoxy propyl alcohol etc.) etc..
In addition, as the polar solvent of aprotic, can include：Acid amides system (N-METHYLFORMAMIDE, N, N- dimethyl
Formamide, N- ethyl-formamides, N, N- diethylformamides, N- methylacetamides, DMAC N,N' dimethyl acetamide, N- ethyls
Amine, N, N- diethyl acetamides, hexamethyl phosphoramide etc.), lactone (gamma-butyrolacton, δ-valerolactone, gamma-valerolactone etc.), ring
Fourth sulfone system (sulfolane, 3- methyl sulfolanes, 2,4- dimethylsulfolanes etc.), cyclic amide system (METHYLPYRROLIDONE
Deng), carbonates (sub- isobutyl ester of ethylene carbonate, propylene carbonate, carbonic acid etc.), nitrile system (acetonitrile etc.), sulfoxide system (dimethyl
Sulfoxide etc.), 2- imidazolones system [1,3- dialkyl group -2- imidazolones (1,3- dimethyl-2-imidazolinones, 1,3- diethyl -
2- imidazolones, 1,3- bis- (n-propyl) -2- imidazolones etc.), 1,3,4- trialkyl -2- imidazolones (1,3,4- trimethyls -
2- imidazolones etc.)] etc..When wherein, using gamma-butyrolacton, ethylene glycol, sulfolane, the characteristic of electrolytic capacitor is good, therefore
It is preferred that.In addition, water can also be contained in a solvent.
It should be noted that in the case of using the much less first alcohols of the carbon numbers such as ethylene glycol as solvent, sometimes by
The phosphoric ester amides that above-mentioned formula (1)~(4) are represented are difficult to dissolve.In this case, bigger by the way that carbon number is applied in combination
Protic polar solvent or aprotic polar solvent, it is possible to increase the dissolubility of phosphoric ester amides.
(di-phosphate ester anion)
In addition, the electrolytic capacitor of the present invention can contain the di-phosphate ester represented by above-mentioned formula (5) in the electrolytic solution
Anion.The di-phosphate ester anion is same with phosphoric ester amides to be difficult to hydrolyze, and with flame retardant effect, therefore, by containing
There is the di-phosphate ester anion, can further improve the anti-flammability of electrolytic capacitor.Particularly with carbon atoms such as ethylene glycol
The phosphoric ester amides that the much less first alcohols of number is represented as solvent, by above-mentioned formula (1)~(4) are difficult in the case of dissolving, such as
Fruit is simultaneously then effective with di-phosphate ester anion.That is, the di-phosphate ester anion represented by above-mentioned formula (5) is easily in ethylene glycol etc.
Dissolving, therefore, by the way that they are applied in combination, can obtain sufficient flame retardant effect.In addition, the di-phosphate ester of formula (5) is cloudy
Ion serves not only as fire retardant and played a role also serving as solute and playing a role, and by adding the di-phosphate ester anion, can drop
The equivalent series resistance (ESR) of low electrolytic capacitor.
In formula (5), Rf1And Rf2Represent that carbon number contains fluoroalkyl or carbon atom for 1~10 straight or branched
Number is the alkyl of 1~10 straight or branched.Wherein, alkyl can be by alkoxy, hydroxyl, amino, N- alkyl aminos, N, N- bis-
The substituents such as alkyl amino, fluorine atom, aryl, sulfanyl, itrile group replace.
As alkyl, for example, can include：Methyl, ethyl, n-propyl, isopropyl, normal-butyl, sec-butyl, tertiary fourth
Base, n-pentyl, n-hexyl, n-octyl, positive decyl etc..As the alkyl after being substituted with a substituent, for example, can include：2-
Methoxy ethyl, 2- hydroxyethyls, 2- amino-ethyls, 2- (N- methylaminos) ethyl, 2- (N, N- dimethylamino) ethyl, 2-
Phenylethyl, 2- methyl thioethyls, 2- cyano ethyls etc..In addition, as fluoroalkyl is contained, for example, can include：Fluoroform
Base, 2- fluoro ethyls, the fluoro ethyls of 2,2- bis-, 2,2,2- trifluoroethyls, the fluoropropyls of 2,2,3,3- tetra-, the fluoropropyls of 2,2,3,3,3- five,
Hexafluoro isopropyl, 2,2,3,3,4,4,5,5- octafluoros amyl group, the difluoro heptyl of 2,2,3,3,4,4,5,5,6,6,7,7- ten, 3,3,4,
Fluorine decyls of 4,5,5,6,6,7,7,8,8,9,9,10,10,10- 17 etc..
In the di-phosphate ester anion of formula (5), in Rf1And Rf2In the case of containing fluoroalkyl, flame retardant effect is excellent,
Particularly double (2,2,2- trifluoro ethyl esters) anion of phosphoric acid are preferred in aspect of performances such as the ESR of anti-flammability and electrolytic capacitor
's.
(adding method)
It should be noted that shown in the di-phosphate ester anion on formula (5), such as following formula (6), with di-phosphate ester (7)
Form contain in the electrolytic solution, ammonia or amine etc. are added in electrolyte progress pH regulations, thus, it is possible to make formula (5)
Di-phosphate ester anion is produced in the electrolytic solution, in addition can also be added the salt (8) of di-phosphate ester in a salt form after preparation
It is added in electrolyte.Here, as salt, can include：Ammonium salt, quaternary ammonium salt, amine salt, season imidazole salts or season amidine salt etc..
(addition)
The addition of the di-phosphate ester anion of formula (5) is not particularly limited, preferably with respect to electrolyte generally 0~
The scope of 50 weight % scope, more preferably 5~25 weight %.Di-phosphate ester anion is relative to electrolyte entirety
When addition is more than 50 weight %, it is possible to be difficult to make proof voltage increase.
(solute)
As solute, organic acid or inorganic acid or its salt can be used alone or in combination.As organic acid, first can be used
The aliphatic monocarboxylic acids such as acid, acetic acid, propionic acid, enanthic acid, malonic acid, butanedioic acid, glutaric acid, adipic acid, methylmalonic acid, heptan two
Acid, suberic acid, azelaic acid, decanedioic acid, dodecanedioic acid, 1,6- decane dicarboxylic acids, heneicosanedioic acid, tridecandioic acid, Malaysia
Aliphatic dicarboxylic acid, benzoic acid, phthalic acid, salicylic acid, toluic acid and the benzene such as acid, citraconic acid and itaconic acid are equal
Aromatic carboxylic acids such as tetracid etc..As inorganic acid, boric acid, phosphoric acid, silicic acid etc. can be used.
As above-mentioned organic acid, the salt of inorganic acid, it can include：Ammonium salt, quaternary ammonium salt, amine salt, season imidazole salts, season amidine
Salt etc..As the quaternary ammonium ion of quaternary ammonium salt, it can include：Tetramethyl-ammonium, triethyl methyl ammonium, tetraethyl ammonium etc..As
The amine of amine salt, can be included：Primary amine, secondary amine, tertiary amine.As primary amine, it can include：Methylamine, ethamine, propylamine etc., as
Secondary amine, can be included：Dimethylamine, diethylamine, ethyl dimethylamine, dibutyl amine etc., as tertiary amine, can be included：Trimethylamine, three
Ethamine, tri-n-butylamine, ethyl diisopropylamine etc..As the season imidazol ion of season imidazole salts, it can include：Ethyl dimethyl
Imidazoles, tetramethyl imidazoles etc..As season amidine, it can include：Ethyl methylimidazole, tetramethyl imidazoles etc..
As long as the concentration of these solutes in a solvent is below saturated concentration.
Furthermore it is possible to above-mentioned di-phosphate ester anion is used alone as solute, can also with organic acid or inorganic acid or
Its salt is applied in combination.
(additive)
In order that the life characteristic of electrolytic capacitor is stabilized, nitrophenol, nitrobenzoic acid, nitrobenzene second can be added
The fragrance such as ketone, nitrobenzyl alcohol, 2- (nitro-phenoxy) ethanol, nitro-anisol, nitrophenetol, nitrotoleune, dinitro benzene
Race's nitro compound.
In addition, the further proof voltage in order to improve electrolytic capacitor, can add nonionic surfactant, incite somebody to action
Polyalcohol and polyoxyalkylene polyol ether compound, polyvinyl obtained from ethylene oxide and/or propylene oxide addition polymerization
Alcohol, polysaccharide (mannitol, D-sorbite, pentaerythrite etc.), complex compound, the cataloid of boric acid and polysaccharide etc..
(anode foils, Cathode Foil, barrier film)
As the anode foils and Cathode Foil of the electrolytic capacitor of the present invention, valve metals such as aluminium, tantalum etc. can be used.Anode foils
In order that increasing with the contact area of electrolyte, it is etched, by chemical conversion treatment, forms oxide film thereon.It is cloudy
Pole paper tinsel can use the electrode foil that implements etching process or without plane paper tinsel for implementing etching process etc., can pass through chemistry
Conversion processing formation oxide film thereon.Barrier film is set between anode foils and Cathode Foil.Here, as barrier film, horse Buddhist nun can be used
Draw the synthetic fibers such as natural fiber barrier film or polypropylene, the polyethylene barrier films such as fiber crops, brown paper or synthetic fibers and natural
Mix barrier film of fiber etc..
(moisture content in element)
Moisture content in the element of electrolytic capacitor is preferably below 10 weight %, more preferably 0.1~8 weight % model
Enclose.When moisture content is more than 10 weight %, it is possible to cause the hydration of electrode foil to deteriorate, thus it is not preferred.By in above range
Interior raising moisture content, can reduce deteriorations of the ESR of electrolytic capacitor without causing electrode foil.In this specification, in element
Moisture be not only to refer to the moisture in electrolyte, and refer to both the moisture that the moisture in electrolyte and element contain.
(manufacture method of electrolytic capacitor)
As the manufacture method of the electrolytic capacitor of the present invention, known method can be used.As one, it can enumerate
Go out：Above-mentioned electrolyte, the side being sealed in external packing box are infiltrated in the element being made up of anode foils, Cathode Foil and barrier film
Method etc..
Embodiment
Hereinafter, embodiments of the invention are illustrated.
(embodiments of the A. on phosphoric ester amides)
The composition of the electrolyte for electrolytic capacitor used in embodiment, comparative example and past case is shown in table 1.It is logical
Cross conventional method and make these electrolyte, ammonia is injected into electrolyte C, adjust pH.Add fire-retardant in the electrolyte of making
Agent is mixed.
Table 1
In the Cathode Foil for implementing the anode foils of etching process and chemical conversion treatment and only implementing etching process
Connection electrode derivation mechanism, across membrane winding, forms element.The electrolyte being produced is infiltrated within the element, is stored
In the external packing box of bottomed tube, the seal formed by elastic caoutchouc is installed in the opening portion of external packing box, passes through constriction
Processing sealing external packing box, makes electrolytic capacitor.
(performance of electrolytic capacitor)
The species, the species of the fire retardant used, resistance of the electrolyte of embodiment 1~3 and past case 1 are shown in table 2
Fire agent relative to the moisture content in the addition of electrolyte, element, the static capacity of electrolytic capacitor, leakage current, ESR survey
Determine result.Used in embodiment 1 as fire retardant in double (2,2, the 2- trifluoro ethyl ester) diethylamides of phosphoric acid, embodiment 2,3
Double (2,2, the 2- trifluoro ethyl ester) diisopropylamides of phosphoric acid have been used, the moisture content in element is changed, does not have in past case 1
There is addition fire retardant.Element as used herein is all using diameter 10mm, length 25mm, 35V-330 μ F element.Leakage current
It is that value under 120Hz, ESR are value under 100kHz to apply the value of 2 minutes, static capacity for voltage.
Table 2
Confirmed by table 2, the electrolytic capacitor of the embodiment 1~3 containing phosphoric ester amides and no addition phosphorus in electrolyte
The past case 1 of ester amides is same, is worked with having no problem as electrolytic capacitor.Particularly in the element of embodiment 2
Moisture content is high, thus, it can be known that compared with embodiment 3 or past case 1, ESR is low, obtains good characteristic.
(self-extinguishment of element)
In the present embodiment, the presence or absence of self-extinguishment by confirming element carries out the checking of anti-flammability.The mechanism that makes to catch fire is approached
The element of electrolyte is impregnated with, is baked 10 seconds on flame, element leaves in the mechanism that makes to catch fire, the presence or absence of self-extinguishment is confirmed.This experiment
In, the mechanism that makes to catch fire is left after element, is judged by the way that whether the burning of element continues more than 10 seconds.Experiment is implemented to each element
3 times.
The species of the electrolyte of embodiment 4~16, past case 2 and comparative example 1~2 is shown in table 3, use it is fire-retardant
The species of agent, fire retardant are relative to the presence or absence of moisture content and self-extinguishment in the addition of electrolyte, element.On self-extinguishment
The presence or absence of, zero symbol represents 3 non-sustained combustions more than 10 seconds, shows with self-extinguishment, × symbol represent 3 times it is lasting
Burning, shows without self-extinguishment.△ symbols represent 1 time or 2 sustained combustions in the experiment of 3 times, show with certainly
The property put out, but it is insufficient.
Double (2,2, the 2- trifluoro ethyl ester) diethylamides of phosphoric acid are used as fire retardant in embodiment 4~7, make electrolyte kind
Class is changed, and the addition of the fire retardant of embodiment 5 is changed in embodiment 8~9, and resistance is used as in embodiment 10~13
Agent is fired using double (2,2, the 2- trifluoro ethyl ester) diisopropylamides of phosphoric acid, Arrays Aluminum Films in Acid Solution is changed, embodiment 14~16
It is middle to use phosphinylidyne N '-methyl piperazine double (2,2,2- trifluoro ethyl esters), diethyl phosphate diethylamide, phosphorus respectively as fire retardant
Using the element with the same composition of past case 1 in sour double (diisopropylamide) 2,2,3,3- tetrafluoro propyl ester, past case 2, compare
It is with the addition of in example 1 as fire retardant in trimethyl phosphate, comparative example 2 and with the addition of triethyl phosphate as fire retardant.In addition, implementing
In example 10 ' and embodiment 10 ", the addition of the fire retardant in embodiment 10 is become respectively and turn to 5%, 30%.
Here, embodiment 6 and embodiment 12 are to use diameter 10mm, the knot of length 20mm, 400V-10 μ F element
Really, in addition embodiment, past case and comparative example is to use diameter 10mm, length 20mm, 35V-330 μ F element
As a result.
Table 3
TMP：Trimethyl phosphate
TEP：Triethyl phosphate
By the results verification of table 3, the past case 2 for not adding fire retardant does not have self-extinguishment, for sustained combustion, real
Applying example 4~16 and comparative example 1~2 has self-extinguishment.But, reduce the embodiment 8 of fire retardant addition, using in ester side
The embodiment 15 of fire retardant without fluorine atom, the embodiment 16 using the fire retardant with 2 amide groups on chain, use phosphorus
Although the comparative example 1 and comparative example 2 of sour trialkyl ester have self-extinguishment, it can not obtain being resistant to the effect of 3 combustion tests.
In addition, by embodiment 10, embodiment 10 ' and embodiment 10 ", double (2,2,2- trifluoro ethyl ester) the diisopropyl acyls of phosphoric acid
The addition of amine is preferably greater than 5 weight % and is below 30 weight %.
(the long-term of self-extinguishment continues)
Species, the kind of the fire retardant used of the electrolyte of embodiment 17~22 and comparative example 3~4 are shown in table 4
Class, fire retardant are relative to the presence or absence of moisture content and self-extinguishment in the addition of electrolyte, element.Embodiment 17 is used and reality
The element of the same composition of example 5 is applied, embodiment 18 makes the moisture content in the element of embodiment 11 be 0.1 weight %, and embodiment 19 makes
Moisture content in the element of embodiment 11 is 10 weight %, and embodiment 20~22 is used and the same composition of embodiment 14~16 respectively
Element, comparative example 3 and comparative example 4 are using the result with comparative example 1 and the element of the same composition of comparative example 2 respectively.
Here, the element used all uses diameter 10mm, length 20mm, 35V-330 μ F element.
Using these elements make electrolytic capacitor, at 125 DEG C it is non-loaded place 500 hours after, from external packing box
Element is taken out, the presence or absence of self-extinguishment is confirmed.
Table 4
The comparative example 3 and comparative example 4 of element with the comparative example 1 of table 3 and the same composition of comparative example 2 have been used first
Phase (table 3) has self-extinguishment, but flame retardant effect disappears in (table 4) after long-time.In contrast, discovery embodiment 17~
22 also have flame retardant effect after long-time.By this as a result, it can be said that the TMP and TEP that are used in comparative example are hydrolyzed, resistance
Fuel efficiency fruit disappears, but embodiment 17~22 is difficult to hydrolyze due to phosphoric ester amides, therefore, also keeps good after long-time
Flame retardant effect.Particularly make the embodiment 19 that the moisture content in element is 10 weight %, even if moisture content in the component compares
In the case of height, anti-flammability is also kept, that is, represents to provide the anti-flammability electrolysis electricity with good characteristic as shown in table 2
Container.
(long-term behaviour of electrolytic capacitor)
Apply 35V voltage in table 5 at 125 DEG C to the capacitor of embodiment 1~3 and past case 1 after 500 hours,
The static capacity of electrolytic capacitor, leakage current, ESR are determined again.In addition, after determining, element is taken out from external packing box, really
Recognize the presence or absence of self-extinguishment.Table 5 is shown in using result as embodiment 1 '~3 ' and past case 1 '.
Table 5
As shown in Table 5, the electrolytic capacitor of embodiment 1~3 not only keeps anti-flammability for a long time, and protects without any problems
Hold electrolytic capacitor performance.
(voltage-resistent characteristic of electrolytic capacitor)
Shown in table 6 make fire retardant species change when electrolytic capacitor voltage-resistent characteristic measurement result.Resistance to electricity
Pressure be the voltage-vs-time when applying constant current (3mA) ascending curve in First Observation to spike or the voltage of flicker
Value.The addition of the fire retardant of embodiment 13 is set to change in embodiment 23 and 24, it is fire-retardant without adding in past case 3
Agent, comparative example 5 changes the Arrays Aluminum Films in Acid Solution of comparative example 2 and the addition of fire retardant.Here, the element used is whole
Use diameter 10mm, length 20mm, 35V-330 μ F element.
Table 6
As shown in Table 6, the electrolytic capacitor of embodiment 23 and 24 with without addition fire retardant past case 3, with the addition of
TEP comparative example 5 is compared, and proof voltage is significantly improved.
It should be noted that in the present embodiment, although used winding shape electrolytic capacitor, but be not limited to this, also may be used
With suitable for stacking shape electrolytic capacitor.
In the present embodiment, the fluorine-containing phosphate ester acid amides as fire retardant is directly with the addition of in the electrolytic solution, but be not limited to
The microencapsulation fire retardant that fire retardant is sealed with the shell materials such as polyphenylene sulfide, can also be added in electrolyte by this.
(embodiments of the B. on di-phosphate ester anion)
The composition of the electrolyte for electrolytic capacitor used in following embodiment and past case is shown in table 7.It is logical
Cross conventional method and make these electrolyte, electrolyte E, F, G, G ', G ", H injection ammonia regulation pH after, further add fire-retardant
Agent is mixed.Electrolyte I is after addition tripropyl amine (TPA) regulation pH, and further addition fire retardant is mixed.Here, electrolyte E,
F, G, G ' mixed solvent of ethylene glycol and diethylene glycol monobutyl ether is used as protic polar solvent, G " is used as protic pole
Property solvent use the mixed solvent of diethylene glycol and diethylene glycol monobutyl ether, electrolyte G, G ', G " is containing phosphoric acid double (2,2,2-
Trifluoro ethyl ester).Electrolyte H is that electrolyte I is to regard gamma-butyrolacton as main solvent as the electrolyte of solvent using ethylene glycol
Electrolyte.
Table 7
In the Cathode Foil for implementing the anode foils of etching process and chemical conversion treatment and only implementing etching process
Connection electrode derivation mechanism, across membrane winding, forms element.The electrolyte being produced is infiltrated within the element, is stored
In the external packing box of bottomed tube, the seal formed by elastic caoutchouc is installed in the opening portion of external packing box, passes through constriction
Processing sealing external packing box, makes electrolytic capacitor.
(performance of electrolytic capacitor)
Shown in table 8 species of the electrolyte of embodiment 25~29 and past case 4, the species of the fire retardant used,
Fire retardant relative to the moisture content in the addition of electrolyte, element, the static capacity of electrolytic capacitor, leakage current, ESR,
The measurement result of self-extinguishment.As fire retardant using double (2,2,2- trifluoro ethyl esters) diisopropyls of phosphoric acid in embodiment 25~29
Acid amides, embodiment 27~29 also contains in double (2,2, the 2- trifluoro ethyl ester) anion of phosphoric acid, past case 4 without addition fire retardant.
The all diameter 10mm of element used herein, length 25mm, 450V-12 μ F element.Leakage current is voltage
The value of application 2 minutes, static capacity is the value under 120Hz, and ESR is the value under 100kHz.In addition, self-extinguishment is as described above, make
Mechanism of catching fire is baked 10 seconds close to the element of electrolyte is impregnated with flame, and the mechanism that makes to catch fire is left after element, passes through element
Whether burning continues more than 10 seconds to judge.Experiment is implemented 3 times to each element, and zero symbol represents 3 non-sustained combustions 10 seconds
More than, with self-extinguishment, × symbol represents 3 equal sustained combustions, without self-extinguishment.△ symbols are represented in the experiment of 3 times
Continue 1 time or 2 times burning, show with self-extinguishment, but it is insufficient.
Table 8
Confirmed by table 8, the electrolytic capacitor of embodiment 25~29 equally has no to ask with past case 4 as electrolytic capacitor
The work of topic ground.In addition we know, the electrolytic capacitor of embodiment 25~29 is compared with the capacitor of past case 4, and self-extinguishment is excellent.
In addition we know, the double weight % of (2,2,2- trifluoro ethyl ester) diisopropylamide 10 of phosphoric acid and phosphorus are contained as fire retardant
The embodiment 27~29 of sour double (2,2,2- trifluoro ethyl ester) both anion, with only containing phosphoric acid double (2,2,2- as fire retardant
Trifluoro ethyl ester) diisopropylamide 10 weight % embodiment 25 compare, anti-flammability is more excellent, with only containing phosphorus as fire retardant
Sour double weight % of (2,2,2- trifluoro ethyl ester) diisopropylamide 18 embodiment 26 is compared, with good ESR values.Need
Bright, the electrolytic capacitor of embodiment 28 is more due to the addition of double (2,2, the 2- trifluoro ethyl ester) anion of phosphoric acid, therefore,
Worked in the case of diameter 10mm, length 25mm, 250V-47 μ F element, but in diameter 10mm, length 25mm, 450V-12 μ F
Element in the case of do not work.
(performance of high voltage electric electrolysis condenser)
Then, in order to compare the performance of high voltage electric electrolysis condenser, as shown in table 9, in embodiment 30, it is used as electrolyte kind
Class uses the electrolyte I containing the gamma-butyrolacton shown in table 7, in addition, using double (2,2, the 2- trifluoro second of phosphoric acid as fire retardant
Ester) diisopropylamide, make electrolytic capacitor.In contrast, in past case 5, being used as Arrays Aluminum Films in Acid Solution shown in table 1
Electrolyte C, does not add fire retardant.In addition, all diameter 10mm of element used herein, length 25mm, 450V-12 μ F
Element.Leakage current is the value that voltage applies 5 minutes, and static capacity is the value under 120Hz, and ESR is the value under 100kHz.Separately
Outside, self-extinguishment is as described above, the mechanism that makes to catch fire bakes 10 seconds on flame close to the element for being impregnated with electrolyte, makes mechanism of catching fire
Leave after element, judge by the way that whether the burning of element continues more than 10 seconds.Experiment is implemented 3 times to each element, zero symbol table
Show 3 non-sustained combustions more than 10 seconds, with self-extinguishment, × symbol represents 3 equal sustained combustions, without self-extinguishment.△
Symbol represents that continuing 1 time or 2 times in the experiment of 3 times burns, and shows with self-extinguishment, but insufficient.
The species of the electrolyte of embodiment 30 and past case 5 is shown in table 9, it is the species of the fire retardant used, fire-retardant
Agent is relative to the moisture content in the addition of electrolyte, element, the static capacity of electrolytic capacitor, leakage current, ESR, self-extinguishment
The measurement result of property.
Table 9
Confirmed by table 9, the electrolytic capacitor of embodiment 30 is same with past case 5, has no as high voltage electric electrolysis condenser
Work to problem.In addition we know, the electrolytic capacitor of embodiment 30 is compared with the capacitor of past case 5, and self-extinguishment is excellent.
(long-term behaviour of electrolytic capacitor)
Then, the electrolytic capacitor and the electrolytic capacitor of past case 5 on above-described embodiment 27,29,30,105
Apply 450V voltage at DEG C after 1000 hours, again the static capacity of measure electrolytic capacitor, leakage current, ESR.In addition,
After measure, element is taken out from external packing box, the presence or absence of self-extinguishment is confirmed.Using result as embodiment 27 ', 29 ', 30 ',
Past case 5 ' is shown in table 10.
Table 10
As shown in Table 10, the electrolytic capacitor of embodiment 27 ', 29 ', 30 ' is compared with the capacitor of past case 5 ', through long
Self-extinguishment is also excellent after time, and electrolytic capacitor performance is also long-term without any problems to be continued.
Claims (7)
1. a kind of anti-flammability electrolytic capacitor, it has：The anode foils, Cathode Foil, barrier film of oxide film thereon are provided with the surface
And the electrolyte containing solute in a solvent, it is characterised in that contain in the electrolyte by following formulas (1) or following logical
The phosphoric ester amides that formula (2) is represented,
In formula (1), n is 1 or 2, R1And R2Alkyl of the carbon number for 1~10 straight or branched is separately represented,
Rf represents the alkane of the straight or branched for being 1~10 containing fluoroalkyl or carbon number for the straight or branched that carbon number is 1~10
Base,
In formula (2), n is 1 or 2, A represent polymethylene that polymethylene, carbon number that carbon number is 4~7 are 4~7
In at least one positions of C-C keys form the groups of C-O-C keys, carbon number for the C-C keys in 4~7 polymethylene extremely
Few 1 position forms at least one position of the group or carbon number of C-NH-C keys for the C-C keys in 4~7 polymethylene
Form C-N (CH3)-C keys group, Rf represent carbon number be 1~10 straight or branched contain fluoroalkyl or carbon number
For the alkyl of 1~10 straight or branched,
Moisture content in the element of the electrolytic capacitor is more than 0.1 weight % and below 10 weight %.
2. anti-flammability electrolytic capacitor according to claim 1, it is characterised in that the phosphoric ester amides are by following formulas
(3) or following formulas (4) represent,
In formula (3), R1’And R2’Alkyl of the carbon number for 1~10 straight or branched is separately represented, Rf ' is represented
Carbon number contains fluoroalkyl for 1~10 straight or branched,
In formula (4), A represents the C-C keys in the polymethylene that the polymethylene that carbon number is 4~7, carbon number are 4~7
At least one position form at least one position of the groups of C-O-C keys, carbon number for the C-C keys in 4~7 polymethylene
Form the group or carbon number of C-NH-C keys and form C-N at least one position of the C-C keys in 4~7 polymethylene
(CH3)-C keys group, Rf ' represent carbon number for 1~10 straight or branched contain fluoroalkyl.
3. anti-flammability electrolytic capacitor according to claim 1 or 2, it is characterised in that integrally contain 5 relative to electrolyte
~30 weight % phosphoric ester amides represented by any one of the formula (1) into (4).
4. anti-flammability electrolytic capacitor according to claim 1 or 2, it is characterised in that also contain in the electrolyte
The di-phosphate ester anion represented by following formulas (5),
In formula (5), Rf1And Rf2Represent the straight or branched that carbon number is 1~10 is 1 containing fluoroalkyl or carbon number
The alkyl of~10 straight or branched.
5. anti-flammability electrolytic capacitor according to claim 3, it is characterised in that also contain in the electrolyte under
The di-phosphate ester anion of formula (5) expression is stated,
In formula (5), Rf1And Rf2Represent the straight or branched that carbon number is 1~10 is 1 containing fluoroalkyl or carbon number
The alkyl of~10 straight or branched.
6. anti-flammability electrolytic capacitor according to claim 4, it is characterised in that relative to electrolyte integrally containing 0~
The 50 weight % di-phosphate ester anion represented by the formula (5).
7. anti-flammability electrolytic capacitor according to claim 5, it is characterised in that relative to electrolyte integrally containing 0~
The 50 weight % di-phosphate ester anion represented by the formula (5).
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| JP2012177768 | 2012-08-10 | ||
| JP2012-177768 | 2012-08-10 | ||
| PCT/JP2013/068064 WO2014024603A1 (en) | 2012-08-10 | 2013-07-01 | Flame-retardant electrolytic capacitor |
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| US (1) | US9496092B2 (en) |
| EP (1) | EP2884511B1 (en) |
| JP (1) | JP6310848B2 (en) |
| KR (1) | KR102085393B1 (en) |
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| KR102098975B1 (en) * | 2012-03-30 | 2020-04-08 | 토소 에프테크 인코퍼레이티드 | Fluorine-containing phosphate ester-amide, and flame retardant resin, flame retardant liquid and flame retardant solvent for oranic synthesis containing same |
| JP6307394B2 (en) * | 2014-09-16 | 2018-04-04 | 東ソー・ファインケム株式会社 | Non-flammable liquid composition comprising phosphoric ester, phosphoric ester amide or phosphoric amide and fluorine-containing phosphoric ester amide |
| CN105403655A (en) * | 2015-12-07 | 2016-03-16 | 山东玉皇新能源科技有限公司 | Method for testing flame retardant property of electrolyte solution |
| CN108110317A (en) * | 2016-11-25 | 2018-06-01 | 深圳新宙邦科技股份有限公司 | A kind of non-aqueous electrolyte for lithium ion cell and lithium ion battery |
| CN107644738A (en) * | 2017-10-17 | 2018-01-30 | 深圳市金元电子技术有限公司 | Boron-free working electrolyte of medium-voltage aluminum electrolytic capacitor for stroboscopic lamp and preparation method thereof |
| US20230327112A1 (en) * | 2020-10-21 | 2023-10-12 | Asahi Kasei Kabushiki Kaisha | Nonaqueous Alkali Metal Power Storage Element and Positive Electrode Coating Liquid |
| CN112582180B (en) * | 2020-11-10 | 2021-11-19 | 西安交通大学 | Electrolyte for high-hydration-resistance medium-high voltage aluminum electrolytic capacitor and preparation method |
| CN114284072B (en) * | 2022-01-07 | 2024-03-29 | 深圳奥凯普电容器有限公司 | Electrolyte for capacitor with wide temperature range, preparation method of electrolyte and capacitor |
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| JPWO2014024603A1 (en) | 2016-07-25 |
| JP6310848B2 (en) | 2018-04-11 |
| WO2014024603A1 (en) | 2014-02-13 |
| KR102085393B1 (en) | 2020-03-05 |
| CN104364861A (en) | 2015-02-18 |
| EP2884511A1 (en) | 2015-06-17 |
| EP2884511B1 (en) | 2019-06-26 |
| US20150325381A1 (en) | 2015-11-12 |
| EP2884511A4 (en) | 2016-03-30 |
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| KR20150040801A (en) | 2015-04-15 |
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